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Article(id=1241799379464552682, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241799375576437302, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.09.010, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1623686400000, receivedDateStr=2021-06-15, revisedDate=1628784000000, revisedDateStr=2021-08-13, acceptedDate=null, acceptedDateStr=null, onlineDate=1773997643580, onlineDateStr=2026-03-20, pubDate=1632067200000, pubDateStr=2021-09-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773997643580, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773997643580, creator=13701087609, updateTime=1773997643580, updator=13701087609, issue=Issue{id=1241799375576437302, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='9', pageStart='1', pageEnd='109', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773997642653, creator=13701087609, updateTime=1773997716115, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241799683752919920, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241799375576437302, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241799683752919921, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241799375576437302, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=65, endPage=68, ext={EN=ArticleExt(id=1241799379821068526, articleId=1241799379464552682, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Influence and Analysis of Nylon Using Red Phosphorus Flame-retardant with Different Coating Process on Electrical Properties of AC Contactor, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

The free acid value and PH3 release amount of PA66 prepared by red phosphorus flame-retardant with different coating process were compared, and the morphology and contact resistance of the corresponding contact element after surface contamination were tested. The effects of housing using different red phosphorus flame-retardant PA66 on the electrical performance of AC contactor were analyzed, and the experiment of simulating the actual application environment was conducted. The results show that the red phosphorus flame-retardant PA66 using multi-layer coating process has low free acid value and PH3 release amount, which has little effect on the electrical performance of AC contactors and can be used as one of the alternative materials for AC contactor housing.

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通过对比不同包覆工艺红磷阻燃剂制备的红磷阻燃PA66的游离酸值与PH3的释放量，以及对应触点元件表面污染后的形貌和接触电阻，分析了使用不同红磷阻燃PA66作为壳体对交流接触器通电性能的影响，并模拟实际使用环境进行了实验。结果表明：使用多层包覆工艺的红磷阻燃PA66的游离酸析出少、PH3释放量低、对交流接触器的通电性能影响较小，可以作为交流接触器壳体的备选材料之一。

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肖体锋（1976-），男（汉族），湖南邵阳人，工程师，主要从事低压电器工控产品的研究和开发设计。

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肖体锋（1976-），男（汉族），湖南邵阳人，工程师，主要从事低压电器工控产品的研究和开发设计。

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肖体锋（1976-），男（汉族），湖南邵阳人，工程师，主要从事低压电器工控产品的研究和开发设计。

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元素质量分数/%原子含量/%
O4.3120.15
Na0.712.31
P5.7013.77
S0.771.79
C0.430.91
Ag88.0861.07
MatrixCorrectionZAF
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通电不良接触器触点元件表面污染物EDX测试结果

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元素质量分数/%原子含量/%
O4.3120.15
Na0.712.31
P5.7013.77
S0.771.79
C0.430.91
Ag88.0861.07
MatrixCorrectionZAF
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项目时间ABC

游离酸值

/(×10-6)

1周235.7223.115.6
2周311.2298.328.5
4周427.3389.739.3

PH3含量

/(×10-6)

1周6.134.120.57
2周15.229.342.61
4周20.6812.723.67
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红磷阻燃PA66游离酸值和PH3含量的对比表

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项目时间ABC

游离酸值

/(×10-6)

1周235.7223.115.6
2周311.2298.328.5
4周427.3389.739.3

PH3含量

/(×10-6)

1周6.134.120.57
2周15.229.342.61
4周20.6812.723.67
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项目接触电阻/mΩ
A-1A-2B-1B-2C-1C-2
实验前8.29.59.87.59.08.3
1周2 6542 8452 1232 0955654
2周2 9573 1542 3952 401145157
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接触电阻对比表

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项目接触电阻/mΩ
A-1A-2B-1B-2C-1C-2
实验前8.29.59.87.59.08.3
1周2 6542 8452 1232 0955654
2周2 9573 1542 3952 401145157
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元素质量分数%原子含量%误差/%
C6.2517.717.07
Ni000
O27.5558.6310.22
P3.533.884.76
Ag62.6719.782.22
Na000
Cu000
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接触器触点元件表面EDX分析（A壳体）

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元素质量分数%原子含量%误差/%
C6.2517.717.07
Ni000
O27.5558.6310.22
P3.533.884.76
Ag62.6719.782.22
Na000
Cu000
), ArticleFig(id=1245084036297769622, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241799379464552682, language=EN, label=Tab.5, caption=EDX analysis of contact element surface for contactor (B housing), figureFileSmall=null, figureFileBig=null, tableContent=
元素质量分数%原子含量%误差/%
C6.8724.416.59
O15.7642.0610.74
P1.952.697.40
Ag72.2128.572.08
Ni2.021.4722.66
Cu1.180.7930.51
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接触器触点元件表面EDX分析（B壳体）

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元素质量分数%原子含量%误差/%
C6.8724.416.59
O15.7642.0610.74
P1.952.697.40
Ag72.2128.572.08
Ni2.021.4722.66
Cu1.180.7930.51
), ArticleFig(id=1245084036465541787, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241799379464552682, language=EN, label=Tab.6, caption=EDX analysis of contact element surface for contactor (C housing), figureFileSmall=null, figureFileBig=null, tableContent=
元素质量分数%原子含量%误差/%
C7.4732.026.95
O6.5421.0612.02
Si1.412.598.27
Ag74.0735.351.97
Ni7.006.148.14
Cu3.512.8415.64
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交流接触器触点元件表面EDX分析（C壳体）

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C7.4732.026.95
O6.5421.0612.02
Si1.412.598.27
Ag74.0735.351.97
Ni7.006.148.14
Cu3.512.8415.64
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尼龙材料采用不同包覆工艺红磷阻燃剂对交流接触器通电性能的影响及分析
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肖体锋 , 胡钰佳 , 章星栋 , 朱映平 , 王剑
绝缘材料 | 材料研究 2021,54(9): 65-68
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绝缘材料 | 材料研究 2021, 54(9): 65-68
尼龙材料采用不同包覆工艺红磷阻燃剂对交流接触器通电性能的影响及分析
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肖体锋, 胡钰佳, 章星栋, 朱映平, 王剑
作者信息
  • 浙江正泰电器股份有限公司，浙江 乐清 325600

    • 肖体锋（1976-），男（汉族），湖南邵阳人，工程师，主要从事低压电器工控产品的研究和开发设计。

Influence and Analysis of Nylon Using Red Phosphorus Flame-retardant with Different Coating Process on Electrical Properties of AC Contactor
Tifeng XIAO, Yujia HU, Xingdong ZHANG, Yingping ZHU, Jian WANG
Affiliations
  • Zhejiang CHINT Electrics Co., Ltd., Yueqing 325600, China
出版时间: 2021-09-20 doi: 10.16790/j.cnki.1009-9239.im.2021.09.010
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摘要
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通过对比不同包覆工艺红磷阻燃剂制备的红磷阻燃PA66的游离酸值与PH3的释放量，以及对应触点元件表面污染后的形貌和接触电阻，分析了使用不同红磷阻燃PA66作为壳体对交流接触器通电性能的影响，并模拟实际使用环境进行了实验。结果表明：使用多层包覆工艺的红磷阻燃PA66的游离酸析出少、PH3释放量低、对交流接触器的通电性能影响较小，可以作为交流接触器壳体的备选材料之一。

交流接触器  /  PA66红磷阻燃  /  无机包覆  /  有机包覆  /  接触电阻

The free acid value and PH3 release amount of PA66 prepared by red phosphorus flame-retardant with different coating process were compared, and the morphology and contact resistance of the corresponding contact element after surface contamination were tested. The effects of housing using different red phosphorus flame-retardant PA66 on the electrical performance of AC contactor were analyzed, and the experiment of simulating the actual application environment was conducted. The results show that the red phosphorus flame-retardant PA66 using multi-layer coating process has low free acid value and PH3 release amount, which has little effect on the electrical performance of AC contactors and can be used as one of the alternative materials for AC contactor housing.

AC contactor  /  red phosphorus flame retardant  /  organic coating  /  inorganic coating  /  contact resistance
肖体锋, 胡钰佳, 章星栋, 朱映平, 王剑. 尼龙材料采用不同包覆工艺红磷阻燃剂对交流接触器通电性能的影响及分析. 绝缘材料, 2021 , 54 (9) : 65 -68 . DOI: 10.16790/j.cnki.1009-9239.im.2021.09.010
Tifeng XIAO, Yujia HU, Xingdong ZHANG, Yingping ZHU, Jian WANG. Influence and Analysis of Nylon Using Red Phosphorus Flame-retardant with Different Coating Process on Electrical Properties of AC Contactor[J]. Insulating Materials, 2021 , 54 (9) : 65 -68 . DOI: 10.16790/j.cnki.1009-9239.im.2021.09.010
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0 引言
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低压电器通常是指在交流电压为1 200 V或直流电压为1 500 V以下工作的电器。常见的低压电器有开关、熔断器、接触器、漏电保护器和继电器等。在电气线路安装时，电源和负载（如电动机）之间用低压电器通过导线连接，可以实现负载的接通、切断、保护等控制功能。交流接触器是常用低压电器之一，其安全性对负载保护至关重要。交流接触器零部件众多，塑料外壳既要起到防护作用，也要对电极进行支撑固定，是交流接触器的核心安全部件，对其主要要求有耐高温、耐电弧灼烧、绝缘、阻燃等。目前行业内用于交流接触器外壳的材料主要有两大类：一类是以酚醛模塑料、不饱和聚酯模塑料等为主的热固性塑料；另一类是以尼龙66（PA66）为主的热塑性塑料。PA66强度高、耐刮擦、可以全自动成型，在数量众多的小规格交流接触器领域应用广泛。普通PA66的阻燃性能较差，通常需要添加红磷、磷氮/氮、溴系阻燃剂等来提升其阻燃性能，其中添加红磷阻燃剂的PA66电气性能优异、耐热性好、性价比高。但使用红磷阻燃PA66制成壳体后，交流接触器偶尔会出现触头电阻增大或者不通电等现象，导致交流接触器的可靠性降低，这是由于交流接触器工作时红磷阻燃PA66中的红磷阻燃剂可能会有不同程度的析出所引起。
对红磷阻燃剂进行包覆处理是解决这个问题的方法之一。包覆红磷全称为微胶囊化红磷，它是近年来广泛应用的一种新型高效、无毒的阻燃剂[1]，其包覆工艺主要分为无机包覆法、有机包覆法、多层包覆法3种。包覆原理是通过物理或化学方法在红磷表面包覆一层或几层连续而致密的无机、有机保护膜，将红磷微粒“包裹”起来，形成微胶囊化红磷阻燃剂。
3种包覆工艺的主要区别如下：①无机包覆法主要采用Al(OH)3、Ti(OH)4-Co(OH)3等材料通过特殊手段沉积于红磷表面，形成无机胶囊状[2]。无机包覆能减缓红磷与空气水分的化学反应，但其具有吸湿性，PH3的释放量较高。②有机包覆法主要采用聚酰胺、环氧树脂、聚氨酯等有机材料作为囊材对红磷进行包覆，包覆效果较好，PH3的释放量比无机包覆法低，但是包覆工艺复杂，成本较高[2]。③多层包覆是先进行无机包覆，然后再选择合适的高分子材料进行有机包覆，这样能大幅降低酸析出的问题[3]。部分材料厂商已有多层包覆技术，能最大限度降低PH3的释放[4]。
本研究对采用不同包覆形式的红磷阻燃剂改性PA66制成的交流接触器[5]进行研究，在模拟实际使用环境下，研究阻燃剂包覆工艺对P元素析出的抑制能力，以及析出物对交流接触器通电性能的影响。
1 实验
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1.1 主要原材料
无机包覆红磷阻燃PA66-GF30-FR(52)，工业品；有机包覆红磷阻燃PA66-GF30-FR(52)，工业品；多层包覆红磷阻燃PA66-GF30-FR(52)，工业品；乙二醇、甲苯、酚酞指示剂，阿拉丁试剂有限公司；银合金触头元件。
1.2 仪器与设备
鼓风干燥箱，DGG-9240B型，杭州卓驰仪器有限公司；恒温恒湿箱，WBE-SDJ型，威邦仪器有限公司；气体检测仪，X-am5000型，德尔格公司；SEM，JSM-IT300型，日本电子株式会社；能量色散X射线光谱仪，EDX-8100型，岛津企业管理（中国）有限公司；直流低电阻测试仪，RDC2511型，杭州威格电子科技有限公司。
1.3 试样制备
1.3.1 标识方法
将无机包覆红磷阻燃PA66-GF30-FR(52)标识为A，有机包覆红磷阻燃PA66-GF30-FR(52)标识为B，多层包覆红磷阻燃PA66-GF30-FR(52)标识为C，对应塑料制件与装配的成品也沿用此标识方法。
1.3.2 制备方法
将3种PA66塑料在120℃鼓风干燥箱中干燥4 h，备用；干燥后的塑料分别注塑成交流接触器壳体，按照标识方法做好标记。成型后的壳体在温度为(23±1)℃、湿度为(50±5)%的标准环境中放置24 h后进行零部件装配，待用。
1.4 测试方法
1.4.1 游离酸值的测试
将称取好的样品浸泡在100 mL溶剂（乙醇和甲苯质量比为1∶1）中，浸泡温度为30℃，浸泡规定时间（实验周期中可间隔取出测试）；将浸泡液过滤至锥形瓶中，用移液管移取25 mL浸出液置于250 mL锥形瓶中，滴加两滴酚酞指示剂，使用10 mL微量碱式滴定管用KOH标准溶液（已用标准邻苯二甲酸氢钾溶液标定浓度）滴定，计算出每克样品消耗KOH的毫克数，记为游离酸值。
1.4.2 PH3含量的测试
将定量样品与10 mL去离子水加入1 L容量的小口磨口瓶中，用真空硅树脂密封后置于70℃烘箱中，达到规定时间后取出，趁热迅速用气体检测仪（PH3检测范围为0～20×10-6，分辨率为0.1×10-6，响应时间为15 s）测定PH3含量，并根据加入的样品量计算材料的PH3含量。
1.4.3 交流接触器接触电阻的测试
常开触头（包括主电路和辅助电路）接触电阻的测试：将线圈通额定电压，产品吸合后，用直流低电阻测试仪的测试夹子分别夹在同相进出线端的两个接触板上，待测试仪显示数据稳定后读数。重复操作3次，以3次中最大值为最后测量值。
常闭辅助触头接触电阻的测试：产品无需通电，用直流低电阻测试仪的测试夹子分别夹在同相进出线端的两个接触板上，待测试仪显示数据稳定后读数。重复操作3次，以3次中最大值为最后测量值。
2 结果与讨论
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2.1 通电不良接触器触点表面分析
对使用有机包覆的红磷阻燃PA66作为壳体而导致通电性能下降的交流接触器进行分析，首先对触点表面进行SEM分析，结果见图1。从图1可以看出，触点表面有大量“树枝状”污染物，这是触点表面存在水分或者在湿度较高的环境下，表面污染物干燥后留下的产物。
对污染物进行EDX分析，结果见表1。从表1可以看出，触点元件表面污染物元素成分主要为Na、S、P。其中Na、S元素来源于海运环境；而P元素则来自于交流接触器自身，交流接触器零部件中只有塑料外壳含有P元素，即红磷阻燃剂。
2.2 红磷包覆工艺对阻燃PA66塑料释放游离酸和PH3的影响
分别称取10 g 3种阻燃剂包覆工艺的红磷阻燃PA66塑料颗粒，各自放置在一个密闭容器中。密闭容器中加入少量纯净水，放在55℃的环境实验箱中进行加速实验。定期测试密闭容器中游离酸值和PH3含量，结果见表2。由表2可以看出，红磷阻燃PA66塑料在高温下会产生游离酸，并且释放出PH3。不同阻燃剂包覆工艺对于抑制游离酸与PH3产生的效果不同，多层包覆工艺的抑制效果显著优于有机包覆，而有机包覆工艺的抑制效果略优于无机包覆。
2.3 红磷包覆工艺对交流接触器接触电阻及触点元件的影响
取3种PA66制得的交流接触器外壳零件A、B、C各两只，装配成交流接触器成品，分别标记为A-1、A-2、B-1、B-2、C-1、C-2，在70℃、90%相对湿度的环境实验箱中进行处理，定期检测交流接触器的接触电阻，实验完毕后检测触头表面的污染物。
2.3.1 交流接触器接触电阻对比
各实验样品处理1周、2周后取出测试接触电阻，结果见表3。从表3可以看出，在高温高湿条件下放置1周后，各交流接触器的接触电阻均有不同程度的上升，以无机包覆红磷阻燃PA66塑料（A）与有机包覆红磷阻燃材料PA66塑料（B）为外壳的接触器的接触电阻均上升约300倍。而以多层包覆红磷阻燃PA66塑料（C）为外壳的接触器的接触电阻虽然也有上升，但是上升幅度相对较小。
2.3.2 交流接触器触头元件表面污染物对比
拆出2.3.1中实验后的接触电阻，各取1只测试完毕的交流接触器触点元件，利用SEM和EDX对触点元件的表面形貌和污染物元素进行分析，结果分别见图2～4和表4～6。对比图2～4和表4～6可以看出，实验后，使用无机包覆红磷阻燃PA66壳体的触头元件表面可见明显污染物，且污染物含有较多的P元素；使用有机包覆红磷阻燃PA66壳体的触头元件表面可见少量污染物，污染物所含P元素亦较少；使用多层包覆红磷阻燃PA66壳体的触头元件表面几乎没有污染物，触头元件表面也未检测到P元素。
交流接触器的工作温度接近70℃，在此温度下，红磷阻燃PA66会产生游离酸，并且释放PH3。PH3在高温高湿的环境下会形成磷酸、亚磷酸等弱酸，金属触点和这些酸在潮湿环境下容易发生化学反应形成盐附着在触电元件表面，导致接触电阻升高。采用多层包覆工艺的红磷阻燃PA66壳体可有效减少游离酸的产生，降低PH3的析出，从而降低触电元件表面接触电阻受潮湿环境的影响。
3 结论
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（1）红磷阻燃剂析出后沉积在触点元件表面形成污染物，是导致交流接触器通电性能下降的主要原因。
（2）在湿热环境下，以不同包覆工艺红磷阻燃PA66塑料为壳体的交流接触器接触电阻均有不同程度的上升，以多层包覆红磷阻燃PA66塑料为外壳的接触器接触电阻的上升幅度相对较小。
（3）不同包覆工艺红磷阻燃PA66在高温高湿的环境下，释放出的游离酸和PH3会附着在元件表面。采用多层包覆工艺可以有效减少游离酸以及PH3的释放量，从而减轻对触点元件的污染。
文献
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参考文献 引证文献
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doi: 10.16790/j.cnki.1009-9239.im.2021.09.010
  • 接收时间：2021-06-15
  • 首发时间：2026-03-20
  • 出版时间：2021-09-20
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  • 收稿日期：2021-06-15
  • 修回日期：2021-08-13
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    浙江正泰电器股份有限公司，浙江 乐清 325600
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Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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